US 11,982,604 B2
Quantification of surface acidity on a low surface area material
Tritti Siengchum, Peninsula, OH (US); and James M Ralph, Copley, OH (US)
Assigned to SAINT-GOBAIN CERAMICS & PLASTICS, INC., Worcester, MA (US)
Appl. No. 17/309,002
Filed by Saint-Gobain Ceramics & Plastics, Inc., Worcester, MA (US)
PCT Filed Oct. 8, 2019, PCT No. PCT/US2019/055088
§ 371(c)(1), (2) Date Apr. 9, 2021,
PCT Pub. No. WO2020/076746, PCT Pub. Date Apr. 16, 2020.
Claims priority of provisional application 62/744,811, filed on Oct. 12, 2018.
Prior Publication US 2022/0026322 A1, Jan. 27, 2022
Int. Cl. G01N 1/40 (2006.01); F01N 11/00 (2006.01); G01N 1/02 (2006.01); G01N 30/72 (2006.01); G01N 33/00 (2006.01); G01N 33/38 (2006.01)
CPC G01N 1/405 (2013.01) [G01N 30/72 (2013.01); G01N 33/0054 (2013.01); G01N 33/388 (2013.01); F01N 11/00 (2013.01); G01N 2001/028 (2013.01)] 11 Claims
OG exemplary drawing
 
1. A method of quantification of surface acidity of a sample, the method comprising the steps of:
(1) removing surface moisture of the sample using a pretreatment process comprising:
heating the sample at about 6-10° C./min, from an initial temperature of about 50-100° C. to about 500-600° C., and
maintaining a temperature of the sample of about 500-600° C. for about 15 to 30 minutes,
wherein the sample is within a Helium or Argon gas flow at a flow rate of about 20-50 cm3/minute;
(2) adsorbing a molecular probe on a surface of the sample comprising:
maintaining a temperature of the sample of about 50-180° C. for about 10 to 20 minutes within a Helium or Argon gas mixed with 5% of the molecular probe flowing at a flow rate of about 10-50 cm3/minute;
(3) removing physically adsorbed molecular probe from the surface of the sample comprising:
maintaining a temperature of the sample of about 50-180° C. for about 60 to 120 minutes within a Helium or Argon gas flow at a flow rate of about 25-50 cm3/minute;
(4) releasing the physically adsorbed molecular probe by a method that includes a temperature programmed desorption (TPD) process comprising:
heating the sample with the molecular probe adsorption at about 6-10° C./min, from an initial temperature of about 50-100° C. to about 500-900° C., and
maintaining a temperature of the sample of about 500-900° C. for about 15 to 30 minutes,
wherein the sample is within a Helium or Argon gas flow at a flow rate of about 20-50 cm3/minute; and
(5) measuring a total amount of the molecular probe physically desorbed from the TPD process by a method that includes mass spectroscopy (MS),
wherein the sample has a surface area to mass ratio of less than 5 m2/g.